Preparation method of palamethasone acetate and palamethasone
A technology of paramethasone acetate and compounds, which is applied in the field of preparation of paramethasone acetate and paramethasone, can solve problems such as insufficient stability of turmeric production, low raw material utilization rate, and fluctuations in raw material prices, and achieve product The effect of increased yield, short reaction route and stable material price
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Embodiment 1
[0041] The preparation of embodiment 1 compound II
[0042] Add 1 part by mass of compound I (16-methylhydroxyl epoxyprogesterone), 3 parts by volume of acetonitrile and 2 parts by volume of pyridine, exhaust the air twice with nitrogen, and stir at room temperature for 10 -15 min, then add 0.5 parts by volume of benzoyl chloride, slowly heat up to 85° C. and react for 4 hours under stirring, and monitor the reaction by TLC. Cool the reaction liquid to 40°C in a cold water bath, then add 1.0 parts by volume of methanol dropwise to the reaction liquid for 10-15 minutes, then continue to react at 40°C for 30 minutes to remove excess benzoyl chloride, and then cool down to -10°C, add 1 volume part of acetonitrile and 0.5 volume parts of water to the reaction solution, stir for 10-15 minutes, add selective fluorine to the above reaction solution in stages, and react for 3 hours until there is a large amount of light yellow Solid precipitated out. In addition, use 0.01 parts by m...
Embodiment 2
[0046] The preparation of embodiment 2 compound III
[0047] Add 1 part by mass of compound II and 8 parts by volume of acetone into the reaction flask, stir for 10-15 minutes, cool to 0-5°C, add 3.5 parts by volume of hydrobromic acid solution dropwise for 30-40 minutes , continue to react for 4.5-h until the solution is clear, and the reaction is monitored by TLC. After the reaction is complete, add 30 parts by volume of water pre-cooled to 0-5°C, dropwise for 40-60 minutes, and dropwise at a temperature of 0-10°C, stir for 1-1.5 hours, precipitate solids, filter, Wash with water until neutral, and dry the solid at 40-50°C for 16 hours to obtain a light yellow bromide solid, namely compound III, with a weight yield of 107% and a product purity of 94.35%. The liquid chromatography data are as follows:
[0048] Table 2. Liquid Chromatography Data for Compound III
[0049]
[0050]
Embodiment 3
[0051] The preparation of embodiment 3 compound IV
[0052]Add 1 part by mass of compound III, 10 parts by volume of tetrahydrofuran, 0.5 parts by volume of tributyltin oxide and 0.5 parts by volume of methylhydrogen silicone oil, and ventilate the air with nitrogen for 2-3 times , and then add 0.02 parts by mass of azobisisobutyronitrile, heat up to 60-65° C. for reflux reaction for 4-6 hours, and monitor the reaction by TLC. After the reaction is complete, cool to 20-40°C, distill under reduced pressure until a large amount of solids precipitate out, about 4-5 parts by volume, add 2 parts by volume of ethyl acetate, continue distillation, and repeat 3 times. Cool to -5-0°C, 3-4h cooling crystallization. Filter, wash with pre-cooled isopropyl ether, and dry the solid at 60-65°C for 24 hours to obtain a slightly yellow debrominated solid, namely compound IV, with a weight yield of 76.80% and a product purity of 96.68%. The liquid chromatography data are as follows surface: ...
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